Process of extracting iodin.



E. HERRMANN. PROCESS OF BETH-ACTING IQDIN. APPLICATION FILED MAY 9, 1906.

' 15,959) Patented Mar. 23,

ERNEST HERRMANN, OF PARKS; FRANCE, ASSZG NOR T COMPAGNIE INTERNATIONALE LA NORG-INE, 0F PARIS, FRANCE.

figaeeifioation 0:2 Letters Fesent.

Patented March 2a, 1909.

I Application filed may 9, 19%, Serial No. 316,002.

by the exhaustion of fresh 'see-Wee(l, dry

sesrweed, see-Weed ,ash or ioduret'l-ed snbstances oi any kind. This exhaustion may be effected in any manner, according to processes already known". if it he desired 'to proceed quiehly, methodical exhaustion with hot water (system of diil'users in sugar workslis advisable. :li cold Water be @1711 ployed it is advisable-in the ease of fresh see,- Weed to destroythe cells, iii-order that the ses-weed may more easily yield it loderetted compounds. The treatment is either effected with a, lime-ni according to ehresdy known processes, or with an acid diluted to 2 to 3 per shoizsond, also eoeording bo-sh'emlyknown processes. 'vntermny indeed be employed. it is only in eesssry to pry shoot 2 g sins more lime ,1; liter in the n r of lime which may eonteln in that case 5 to 7 per thouse n of lime, so 'fio eowipensete the loss of oomposition ofthe i'll'llOllCl. of rnagnes n which gives ehlorid oi calcium and insole magnesia which does no harm. Thus lie; unis are oha'ined whieh according to ere pounds to the extent 05-300 510 1000 grams of iodin per cuhlemeter; These liqu ds they are then conveyed to wooden. vets of medium size,' in which stirring is essilv f 'ieoted, and the iodin set free by on,

knownmeans, sulfuric aoid'or new oi forexemplei The ioduretted eomponnr thus decomposed and she iodin set, free.

liters (or approrcinmtely) of pure VIJLSGliIlG oil I in the Water.

line due to the de-' I iodinv then decent-ed iineees'ssrv or even limitedtially exhausted and poor in iodin, then passes over liquid already once exhausted and finally over e fresh liquid. Thus 95% of 10(lll1 is carried of? =W1i3l1 about 60 liters of Vaseline oil per cubic meter of liquid. This 'Vesehne 011 thus onriehr-ad Wltlh-lmlllfl, IS

poured inbo e stoneware or wooden receptacle and heated directly by 2i current of steam. This receptacle oommunieetes with another similar receptacle through a. porcelain. or lefrigerstor the letter if neoesssry being multituhuler in order to effect adequ see oooling.

The steam begins by heating the oil and the first receptacle must be rather large in order to contain the vapor condensed by'this operation. Then, when the aseline oil is hot, the steam Carries oil the iodin which is 'Slllillifilflhfid and becomes. condensed in the refrigerator. Owing to the action of the steam she refrigerator does not become stopped. The second receptacle on. the oi-her'eide of'bhe refrigerator receives the gem dense/d steam and partieles of iodin carried When the Vaseline oil has films heen deprived of its iodin, it is cooled and, is employed again for treating liquids already mrtioll exhausted. The Vaseline oil ins s so he deprived of its iodin, red,bybeingdirectlyheated or by ecifed by a current of hot air or of an inert I? it he desired to proceed ifiore quickly "with. the removal of the iodin from the vaseiili'ie oil so thst a smaller enormity of Vaseline oiigwill he required for the whole treatment, the} iodin may he exhausted from the vaseh'nd oil itself by stirring the oil with 9, liquideepsf'ole of formingn combination with the This result may he obtained very quickly with $1, solnnion of potash or of soda; hes a certain time is required for decanting.

- The solution of sulfite of sods, while not taking more time to absorb the iodin, allows of very quick decanting. I The operation may proceed as follows 1- o 600 parts of ioduretted VfiLSOllDO oil, 1000 isrfis of Water oonteining an excess of Slllfitare ended, stirring being carried on untll the color due to the iodin has (lien )peared. The Vaseline is decanted, remove by an equal uentity of ioduretted Vaseline oil Thus Will the seine 1 non tity of liquid, to which when necessary sulfite is again added, it'is possible to exhaust to volumes snd replacedployed (this being of Vaseline oil, thus enabling a highly con- 'centrated iodid liquor to be obtained. The

iodin of these concentrated liquors-is set free by the known means, nitrites or chlorates,

by being drawn off by process is obtained from thepetroleum of bralicia (Austria); it constitutes a neutral uncolored liquid which distils only at a temerature above 350 degrees Celsius (660 F.). This vaseline oil appertains to the chemical groupof parafiins it is not oxidized by contact with air, and it is not affected by the presence of concentrated acids.

The employment of Vaseline oil insures the following advantages: The oil does not evaporate and does not ignite like beirzene, petroleum or the like it floats on .the surface, thus enabling more or less clearr liquids to be emimpossible with solvents eavier than Water, such as carbon bisulfid, chloroform or tetrachlorid of carbon), without washing and without subsequent treatment; it distils at about 345 degrees centi grade, thus enabling steam to be employed, as it does not emit any vapor before reaching its point of distillation. Finally the chemical group to which it belongstheparafiins are insensible to reagents and non-oxidizable in tllle air and thus can be employed indefinite y.

An apparatus for carrying out the process is shown in sectional elevation in the accompanying drawings. 7 In this Figure 1 is a receptacle of wood or is to be extracted; 2 is a similar receptacle containing pure vaseline oil 3 is a wooden vat provided with a stirring the process already deapparatus il-actuated by any wellsumac known means; 5 is a tube or pipe for supplying the liquid contained in the receptacle '1 to the vat 3; 6 is another pipe by means of which the pure vaseline oil contained in the reqepv tacle 2 is discharged to the bottom of the'vat 3. The oil enriched with iodin collects on the surface and is discharged continuously by the tube 7, into the stone-ware receptacle 1031111 a kind of sprayer for the exit of steam.

The receptacle 8 communicates with the second rece tacle 10 by means of a tube 1 1, preferably of porcelain or glass for the escape of the steam carr ing 0 the iodin which is sublimated. I T e refrigeration is obtained by cold water, furnished by a tank 12 which communicates with the refrigerating jacket 13, by means of the pipes .14 and 15, arranged in the manner shown in the drawing for obtaining a continuous flow of cooling water. The arrows-inthe drawing show the directions in which the fluids move in the difierent tubes and receptacles.

Having now described my invention, what I claim as new and desire to secure by Letters Patent is:

A process of extracting iodin consisting in first liberatin the iodin from iodin lyes, then mixing t e iodin liquid with vaseline oil and then obtaining pure iodin directly from the resultant solution by subliming with steam.

In testimony whereof I have signed my I name to this specification in the presence of 1 two subscribing witnesses.

other convenient material for containing the liquids from which iodin ERNEST HERRMAN N.

W'itnesses: v I

ERIK T. BECKER, Jr. HANSON O. Coxn. 

